Method of treating pectin-containing raw material



1 mi us Jilly 11 193 9 a a r 2,165,902

UNITED STATES PATENT OFFICE r rs'rnon or manner; rsc'rm-con'rsmmo aaw MATERIAL Philip Bliss My ers, Scarsdale, N. 2., assignor to Sardik Incorporated, Jersey City, N. J., a corporation of Delaware No Drawing. Application January 18, 1938, v

' Serial No. 185,520

11 Claims- (choc-21o) This invention relates to the treatment of a method of treating pectin-containing raw ma- 7 pectin-containing raw material, and an object terial which will not only overcome, the memis. to provide a method of conserving the jelly ciencies in and objections to customary methods units and preventing lossor deterioration of the of treatment heretofore in use, but will enable pectin in such raw material during the handling the material to retain substantially its full avall- 5 and storage thereof. able pectin content without any substantial loss The main source of pectin is now either the of jelly units during the handling and storage residue from cider mills known as apple pomace, thereof. a or the white rind or peel oi citrusv fruits known These and other objects which will be appar-. as albedo. Such raw material can be obtained exit to those skilled in the art are attained by 10 in commercial quantities only during a relatively means of the present invention, one embodiment few months of the year. when the fruit is ripenof which is hereinafter described by way of ing. Apple pomace is obtalnableonly when the example. cider mills are operating. Albedo is obtainable In carrying out this invention the raw mate-' [I only when the canneries or citric acid plants rial is subjected to a treatment in which the i5 are operating. The. latter, for example, operate water soluble pectin present is rendered insolonly from three to four months of the year. uble and resistant to those dete crating, influ- Hence, a year's supply of pomace or albedo to ences usually encountered in th handlingand be used in preparing pectin must be acquired storing of the material. is accomplished during a relatively short period in each year by treating the raw material with copper which 20 and stored for subsequent use. combines with the pectin present to form an when received. the vraw material, either alinsoluble copper pectinate. when so treated'the' bedo or pomace, is usually ground and then kiln material can be dried, in any desired manner, dried. As no impurities are removed during. and stored for extended periods without sui'ier- 25 these operations, the resulting producteis susing deterioration and without requiring cold 25 ceptible-to fermentation with consequent loss of storage. When wanted for use the metal can be jelly units. For example, in the case-oi apple easily eliminated "by washing the material in a pomace which contains a relatively high persuitable bath. oentage of fruit sugars, it is necessary to place The raw material is first mound to approxithe material in cold storage immediately after mat ly %"*-'/a" Siz Wh it is as f h p 30 drying in ordr to prevent-spoiling due to Iersible. The ground material is then leached or mentation. washed with a dilute copper salt solution, pref- Also, the raw material contains the enzyme erably a solution of copper-s ph which i pectinase which breaks down the pectin and heated to a sumcient temperature to render the causes a loss of jelly units. This enzyme can enzyme Pfictinase inactive. after which the raw 36 be rendered inactive by heating the material to m r l is separated im dr e certain temperatures but this must be done im- In leaching, about 2.5 pounds oi! water should mediately upon the material being ground or be employed for each pound of ground raw maelse a large percentage of jelly units will be lost. terial, and enough copper saltused to provide 40 The ordinary kiln drying oi the material is necapproximately one pound of, copper in the leacho essarily so slow that the material is not heated ing water to each 18 pounds or water soluble to the required temperature quickly enough to pectin present in the raw material. prevent a substantial loss of jellyunits. The percentage of water soluble pectin pres- As the season advances, that is to say, as-the ent in any given batch of raw material can be fruit ripens, the amount of water soluble pectin readily determined by well-known laboratory 5 present'increases rapidly. Inasmuch as pomac'e tests. and albedo are not available until the season For example, assume one thousand (i000) g is well advanced it is practically impossible to pounds of ground grape truit peel is being obtain raw material without a large percentage treated. and that tests show the peel to contain o! water soluble pectin. As is well known',*such 3.5% pectin of which approximately 40% is wapectin deteriorates rapidly under the influence ter soluble. In other words, one thousand (1000) or heat so that the customary kiln drying operapounds or such albedo contain approximately 14 )ilon above referred to destroys a large and valupounds or water'soluble pectin. A leaching bath able part of the otherwise available pectin. is prepared by providing approximately 2500 q. Aturther object 01 this invention is to provide pounds of water in a suitable tank preferably 5 having a false bottom. Copper in the form of a soluble copper salt is added to the water in suilicient quantities to provide approximately 1 pound of copper to every 18 pounds of water soluble pectin. In the present illustration, assuming that'copper sulphate, CuSO4.5H2O, is employed, approximately 3.06 pounds of salt containing approximately 0.78 pound of copper is added and the bath heated to boiling.

As soon as the albedo is around it is dumped into the boiling water and vigorously agitated. This introduction of the cold material into the bathwill reduce the temperature thereof to a point below 90 C., the temperature at which the enzyme pectinase is rendered inactive. Accordingly, it is necessary to continue heating the bath in order to raise its temperature as rapidly as possible to approximately 90 C. and maintain it at that temperature for from 5 to 10 minutes.

Heating is then discontinued and the batch rapidly cooled to from 50 to 60 C., preferably by introducing approximately 2500 pounds of cold Water into the bath. Upon cooling the bath is stirred for approximately minutes after which the water is drained off through the false bottom and the residue, that is to say the pectin-containing raw material is dried in a kiln or in any other suitable form of drying apparatus.

Although the volumes of water given in the above example are not critical in any sense, the exact amount of water employed being relatively unimportant, it is advisable to use sufflcient, water to insure removal of most of the soluble constituents offthe raw material.

It will be found that copper has combined with the soluble pectin present in the raw material so that the mount of copper in the leached material so treated is substantially non-hygrouble pectin present in the raw material. The material so treated is subtantially non-hygroscopic and the pectin is so stable that it can be dried over a period of two or three days in ordinary shelf driers and then kept for prolonged periods without loss of jelly units and without requiring refrigeration. As the material is not slimy, a much greater percentage of water can.

be removed by pressing than has heretofore been possible. For the same reason, the material can be more easily dried in a kiln as itwill not stick to the sides thereof and being of lower moisture content can be dried at lower temperatures and therefore more economically than has heretofore been possible. As a matter of fact, any desired type of drying in addition to kiln drying can be employed without injuring the pectin content.

Also, as a result of the present process, the soluble constituents of the raw material are removed substantially without loss of soluble pectin so that after the leached material is dried it contains from to of pectin. This removal of impurities from'the pectin-containing raw material constitutes an important advantage which is gained by the present invention. These impurities normally include invert sugars, acids, salts, oils, tannins and so forth. When present,

being hygroscopic, they not only render thematerial diillcult to dry, but after drying result in taking up moisture from the atmosphere. Heretofore, so far as I know, it has been impossible to remove these impurities previous to drying because at the same time the soluble pectin would be lost. However, as a result of the present process, the soluble pectin is retained in the material while the impurities are removed in the leaching operation. As a result, it will be found much easier to dry the raw material and at lower temperatures. Removal of the impurities increases the percentage of pectin in the dry material and reduces the weight of material which has to be stored. The enzyme pectinase has also been rendered inactive without loss of soluble pectin. Pectin extracts made from raw material treated in accordance with the present invention can be more easily clarified because of the less slimy quality of the extract obtained from such material.

The invention can be variously modified and adapted within the scope of the appended claims.

I claim:

1. That step in the process of treating pectincontaining raw material which consists in leaching the material with a copper salt solution to form an insoluble copper pectinate.

2. That step in the process of treating pectincontaining raw material which consists in leaching the material with a'solution of copper sulphate containing sufilcient copper to combine with-susbtantially all soluble pectin present to form an insoluble copper pectinate.

3. The process of treating pectin-containing raw material which consists in grinding the material, leaching the material with a copper sulphate solution to transform the pectin into a copper pectinate, heating during the leaching operation, separating out the leached material and drying. 1

4. The process of treating material containing water soluble pectin which comprises washing the material with a solution of a copper salt to transform pectin into an insoluble copper pectinate, and simultaneously heating the material to a temperature sufllcient to inactivate the enzyme pectinase.

5. The process of treating material containing water soluble pectin which comprises washing the material with a solution of a copper salt to transform pectin into an insoluble copper pectinate, and simultaneously heating the material to 90 C. to inactivate the enzyme pectinase.

6. The process of treating pectin-containing raw material which comprises grinding the material, leaching the material with a solution of a copper salt heated to approximately 90 C. to transform the pectin into a. copperv pectinate.

separating the material therefrom and agai heating the material to dry the same.

7. The process of treating pectin-containing raw material which consists in grinding the raw material, leaching the material in a copper salt solution comprising approximately 1 pound of copper to each 18 pounds of soluble pectin present in said raw material to transform the pectin into an insoluble copper pectinate.

8. The process of treating pectin-containing raw material which consists in grinding the raw material, leaching the material in a copper salt solution comprising approximately two and onehalf parts of water to each part of raw material and approximately 1 pound of copper to each 18 pounds of soluble pectin present in said raw material to transform the pectin into an insoluble copper pectinate and to,remove the soluble impurities-therefrom.

9. The process of treating pectin-containing raw material which comprises grinding the material, leaching the material with a copper sulphate I solution heated to approximately 90 C., to transform the pectin into an insoluble copper pectinate, separating the material therefrom and again heating the material to dry the same.

moaooa 10. The process of treating pectin-containing raw material which consists in grinding the material, leaching the material in a copper sulphate solution comprising approximateLy two and onehalt parts of water for each part of raw material and suflicient copper sulphate to provide approximately 1 pound of copper to each 18 pounds of soluble pectin present in said raw material to transform the pectin into an insoluble 10 copper pectinate, heating the solution suiiiciently to render the enzyme pectinase inactive, then separating the material from the solution, and again heating the material to dry the same.

11. A process of treating pectin-containing raw material which consists in treating the material with a copper salt in sufllcient quantity to ,react with substantially all soluble pectin present to form an insoluble copper pectinate, separating out the leached material, and drying. PHILIP BLISS 

